量子电子学报, 2010, 27 (1): 110, 网络出版: 2010-05-31   

尿素共沉淀法制备Nd:YAG纳米粉体

Preparation of nanoscaled Nd:YAG powders by the urea co-precipitation method
作者单位
中国科学院安徽光学精密机械研究所,安徽省光子器件与材料重点实验室, 安徽 合肥 230031
摘要
采用共沉淀方法,以 Nd2O3、Y2O3和Al(NO3)3?9H2O为起始原料, 尿素为沉淀剂,制备Nd:YAG纳米粉体,粉体经 XRD、TG-DTA、FESEM 以及激光散射等测试手段对其结构和形貌进行测试研究。XRD 表明,前驱体在900 ℃煅烧3 h 出现了 YAG 相和 YAM 中间相,在1000 ℃及其以上煅烧3 h后已完全转变成YAG 相,且随着煅烧温度升高,衍射峰逐步增强, 900 ℃~1200 ℃煅烧的 Nd:YAG 晶格常数值从 1.2012 nm变化到 1.1994 nm,颗粒度从 31 nm变化到 96 nm,激光粒度仪也给出了 类似的变化趋势。TG-DTA 结果表明当前驱体加热到 1200 ℃时,粉体总重量损失约为43%。对前驱体进行了水洗和乙醇洗两种洗涤, 比较发现乙醇洗涤更有利于 Nd:YAG 纳米粉体的分散,这些实验结果可为制备优良YAG透明陶瓷粉体提供参考。
Abstract
Nd:YAG nanoscaled powders were prepared by the co-precipitation method with Nd2O3, Y2O3 and Al(NO3)3?9H2O as the starting materials and CO(NH2)2 as the precipitator. The structure and morphology of the powders were investigated by XRD, TG-DTA, FESEM and laser particle analyzer. XRD patterns show that YAG phase and intermediate phase YAM were detected in the sample from the precursor calcined at 900 ℃ for 3 hours, the precursor completely transformed to YAG phase when it was calcined at 1000 ℃ for 3 hours, and the intensity of YAG X-ray diffraction peaks increased with the increase of calcination temperature. Lattice parameters of Nd:YAG phase calcined at 900 ℃~1200 ℃ changed from 1.2012 nm to 1.1994 nm, and the particle size ranged from 31~96 nm. The similar variation was given by a measure of laser particle analyzer. The TG-DTA results indicate that the mass loss value was about 43% when the precursor was heated up to 1200 ℃. Suspension was washed with distilled water and alcohol, respectively. The comparison results show that alcohol is more effective for the well-dispersion of the nano-sized Nd:YAG powders. The results provid references for preparing good powders of YAG transparent ceramics.

李冬青, 丁丽华, 张庆礼, 邵淑芳, 宁凯杰, 殷绍唐. 尿素共沉淀法制备Nd:YAG纳米粉体[J]. 量子电子学报, 2010, 27(1): 110. LI Dong-qing, DING Li-hua, ZHANG Qing-li, SHAO Shu-fang, NING Kai-jie, YIN Shao-tang. Preparation of nanoscaled Nd:YAG powders by the urea co-precipitation method[J]. Chinese Journal of Quantum Electronics, 2010, 27(1): 110.

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